2.7 Experimental Section
55
Table 2.4 (continued)
Compound
3/DMA
3/AcH
3/CH 3 CN
3/DMF
Max./Mini.
peak I d (Å 3 )
1.32 e − /−1.10 e −
1.25 e − /−1.07 e −
2.36 e − /−2.24
e −
3.02 e − /−2.90 e −
Compound
3/SPO
3/racPO
3/acetone
3/none
CCDC
number
1486484
1486483
1486475
1486485
Empirical
formula
C 29 H 24 Au 2 N 2 O C 26.75 H 19.5 Au 2 N 2 O 0.25 C 26.75 H 19.5 Au 2 N 2 O 0.25 C 26 H 18 Au 2 N 2
Formula
weight
810.45
766.89
766.89
752.27
Crystal
system
triclinic
monoclinic
monoclinic
monoclinic
Crystal size
(mm)
0.466 × 0.226
× 0.211
0.162 × 0.137 × 0.123
0.565 × 0.072 × 0.054
0.141 × 0.071
× 0.058
a (Å)
13.9136(9)
14.2069(14)
13.6877(11)
14.0825(19)
b (Å)
14.8769(9)
22.8755(17)
26.0965(17)
13.9789(14)
c (Å)
15.0369(9)
14.8349(11)
26.9019(19)
21.934(2)
α (°)
78.416(3)
90
90
90
β (°)
65.9278(14)
95.445(4)
90.5498(19)
92.577(6)
γ (°)
63.373(5)
90
90
90
V (Å 3 )
2539.8(3)
4799.4(7)
9608.9(12)
4313.5(9)
Space group
P1 (#1)
I2/a (#15)
P2 1 /n (#14)
I2/a (#15)
Z value
4
2
2
8
D calc
(g cm −3 )
2.119
2.123
2.140
2.317
Temperature
(K)
123
123
123
123
2θ max (°)
52.0
51.0
55.0
50.1
μ(Mo K α )
(cm −1 )
116.037
122.723
122.567
136.516
No. of
reflections
Total: 21,049
Unique: 15,961
R int = 0.0830
Total: 17,826
Unique: 4377
R int = 0.1430
Total: 87,827
Unique: 21,691
R int = 0.2838
Total: 16,641
Unique: 3817
R int = 0.2236
R a
1
0.0850
0.0860
0.0934
0.0925
wR b
2
0.2511
0.2474
0.2736
0.2856
GOF c
1.124
1.045
0.903
1.017
Max./Mini.
peak I d
(Å 3 )
6.69 e − /−4.66
e −
3.89 e − /−2.53 e −
1.94 e − /−2.13 e −
2.20 e − /−1.78
e −
a I > 2.00σ(I)
b All reflections
c Goodness of Fit Indicator
d In Final Diff. Map
55
Table 2.4 (continued)
Compound
3/DMA
3/AcH
3/CH 3 CN
3/DMF
Max./Mini.
peak I d (Å 3 )
1.32 e − /−1.10 e −
1.25 e − /−1.07 e −
2.36 e − /−2.24
e −
3.02 e − /−2.90 e −
Compound
3/SPO
3/racPO
3/acetone
3/none
CCDC
number
1486484
1486483
1486475
1486485
Empirical
formula
C 29 H 24 Au 2 N 2 O C 26.75 H 19.5 Au 2 N 2 O 0.25 C 26.75 H 19.5 Au 2 N 2 O 0.25 C 26 H 18 Au 2 N 2
Formula
weight
810.45
766.89
766.89
752.27
Crystal
system
triclinic
monoclinic
monoclinic
monoclinic
Crystal size
(mm)
0.466 × 0.226
× 0.211
0.162 × 0.137 × 0.123
0.565 × 0.072 × 0.054
0.141 × 0.071
× 0.058
a (Å)
13.9136(9)
14.2069(14)
13.6877(11)
14.0825(19)
b (Å)
14.8769(9)
22.8755(17)
26.0965(17)
13.9789(14)
c (Å)
15.0369(9)
14.8349(11)
26.9019(19)
21.934(2)
α (°)
78.416(3)
90
90
90
β (°)
65.9278(14)
95.445(4)
90.5498(19)
92.577(6)
γ (°)
63.373(5)
90
90
90
V (Å 3 )
2539.8(3)
4799.4(7)
9608.9(12)
4313.5(9)
Space group
P1 (#1)
I2/a (#15)
P2 1 /n (#14)
I2/a (#15)
Z value
4
2
2
8
D calc
(g cm −3 )
2.119
2.123
2.140
2.317
Temperature
(K)
123
123
123
123
2θ max (°)
52.0
51.0
55.0
50.1
μ(Mo K α )
(cm −1 )
116.037
122.723
122.567
136.516
No. of
reflections
Total: 21,049
Unique: 15,961
R int = 0.0830
Total: 17,826
Unique: 4377
R int = 0.1430
Total: 87,827
Unique: 21,691
R int = 0.2838
Total: 16,641
Unique: 3817
R int = 0.2236
R a
1
0.0850
0.0860
0.0934
0.0925
wR b
2
0.2511
0.2474
0.2736
0.2856
GOF c
1.124
1.045
0.903
1.017
Max./Mini.
peak I d
(Å 3 )
6.69 e − /−4.66
e −
3.89 e − /−2.53 e −
1.94 e − /−2.13 e −
2.20 e − /−1.78
e −
a I > 2.00σ(I)
b All reflections
c Goodness of Fit Indicator
d In Final Diff. Map